CN109439015A - A kind of permanent bordeaux pigment and preparation method thereof suitable for baking finish - Google Patents
A kind of permanent bordeaux pigment and preparation method thereof suitable for baking finish Download PDFInfo
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- CN109439015A CN109439015A CN201811397633.5A CN201811397633A CN109439015A CN 109439015 A CN109439015 A CN 109439015A CN 201811397633 A CN201811397633 A CN 201811397633A CN 109439015 A CN109439015 A CN 109439015A
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- parts
- baking finish
- permanent bordeaux
- preparation
- coupling
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B29/00—Monoazo dyes prepared by diazotising and coupling
- C09B29/10—Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group
- C09B29/18—Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group ortho-Hydroxy carbonamides
- C09B29/20—Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group ortho-Hydroxy carbonamides of the naphthalene series
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- Organic Chemistry (AREA)
- Cosmetics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The permanent bordeaux pigment and preparation method thereof that the invention discloses a kind of suitable for baking finish.This kind of pigment improves whole system by the way that surfactant polyoxyethylenealkylphenol ether is added, and makes it in the application and preparation of baking finish, has preferable dispersibility, can preferably and media compatibility, to increase the stability and storage time of baking finish finished product.
Description
Technical field
The present invention relates to technical field of chemical pigments, and in particular to a kind of suitable for the permanent bordeaux pigment of baking finish and its preparation
Method.
Background technique
It is higher and higher to the demanding criteria of pigment now with the development of science and technology, especially dispersion performance application side
Face is also continuously improved, the application especially in baking finish, and major part permanent bordeaux pigment compatibility in using medium is bad at present, makes
It is short with the stability and period of storage of baking finish finished product.
Summary of the invention
It is an object of the present invention in view of the above shortcomings of the prior art, propose a kind of permanent bordeaux face suitable for baking finish
Material and preparation method thereof, this kind of pigment have good dispersibility, can be good compatible with the medium in baking finish.
A kind of permanent bordeaux pigment suitable for baking finish proposed by the present invention includes following component: color base 15-25 by weight
Part, 20-30 parts of Naphthol AS-PH, sub- 15-30 parts of sodium, 7-10 parts of liquid alkaline, 15-20 parts of hydrochloric acid, polyoxyethylenealkylphenol ether 2-4
Part, 3-8 parts of diatomite, 2-5 parts of sulfamic acid and 3-7 parts of auxiliary agent.
It further, further include 60-80 parts and ice 45-60 parts of water.
Further, the color base includes RC35-50 parts and large red-based g 10-25 parts of erie Congo base by mass parts.
Further, the auxiliary agent includes 2-3 parts and polysorbas20 1-4 parts of sodium metnylene bis-naphthalene sulfonate by mass parts.
Further, the carboxyl in negative point is introduced in the polysorbas20 molecule.
Further, the sub- sodium is one of sodium nitrite and sodium sulfite or two kinds
A kind of preparation method of the permanent bordeaux pigment suitable for baking finish, comprising the following steps:
(1), the preparation of diazo liquid: it is separately added into color base, auxiliary agent and sub- sodium in acidic environment, diazo reaction occurs, obtain diazonium
Liquid；
(2), the preparation of coupling solution: azoic coupling component, liquid alkaline and diatomite are added into water, obtains coupling solution after to be dissolved；
(3), it is coupled: after coupling solution, polyoxyethylenealkylphenol ether, sulfamic acid is added into diazo liquid, being coupled, obtained
Coupling product；
(4), it keeps the temperature: coupling product being kept the temperature, product is obtained after heat preservation.
Further, whole process needs lasting stirring, stirring rate 40HZ in step (1), and coupling solution temperature is 5-
10℃。
Further, solution temperature is 45-50 DEG C in step (2), and the dissolved stand-by temperature of preservation is 38-42 DEG C.
Further, the coupled processes pH in step (3) is to add azoic coupling component, pH after diazonium disappears less than or equal to 4.2
For 3.8-4.0.
A kind of permanent bordeaux pigment and preparation method thereof suitable for baking finish of the invention, this kind of pigment are living by the way that surface is added
Property agent polyoxyethylenealkylphenol ether improve whole system, make it in the application and preparation of baking finish, have preferable point
Property is dissipated, it can preferably and media compatibility, to increase the stability and storage time of baking finish finished product.
Specific embodiment
For present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, various changes or modification that those skilled in the art make the present invention, this
A little equivalent forms are equally fallen in the application range claimed.Proportion in the embodiment of the present invention is by weight.
Embodiment 1
Diazo liquid preparation:
It discharges water in diazonium bucket, hydrochloric acid is added, open stirring adjustment motor speed 40HZ, erie Congo base RC35 parts and large red is added
G10 parts of base, 2 parts of sodium metnylene bis-naphthalene sulfonate and 1 part of polysorbas20 stir 15 minutes (inspection is completely dissolved transparent), temperature 25
Degree.Ice adjustment temperature T=0 DEG C is added, sub- 15 parts of sodium is added.It (is detected with KI test paper in the case where keeping the micro- excessive situation of sub- sodium
Micro- aobvious blue) stirring 30 minutes, temperature is controlled at 5 DEG C.Volume 6500L, wait be coupled.
Coupling solution preparation:
Water 5700L is added in dissolving bucket, opens stirring adjustment motor speed 40HZ, is warming up to 45 DEG C with steam, adds azoic coupling component
20 parts of AS-PH, 7 parts of liquid alkaline are added, is dissolved 20 minutes, whether detection dissolution is transparent, and dissolution is fully transparent, and diatomite 3 is added
Part, add 1500 L of water to adjust 40 degree of temperature, wait be coupled.
Coupling and heat preservation:
7500 L of water is added in coupling bucket, opens stirring, adjusts motor speed 25HZ, has corrected acidometer, sequentially added liquid alkaline 7
Part and 2 parts of polyoxyethylenealkylphenol ether, pH=4.0, then adjustment temperature on the rocks is to 8 DEG C.Diazo liquid is put into coupling bucket again, pH=
1.6, it is adjusted with 2 parts of sulfamic acid micro- excessive or not excessive to sub- sodium.
Coupling is pumped into filter press to be filtered, then it is added to coupling bucket in a manner of being coupled under liquid, adjustment motor turns
Fast 50HZ starts to be coupled.Coupling time requires to be 1.5 hours.It is coupled start temperature and requires 10 DEG C, terminating temperature requirement is about 25
DEG C (if room temperature is too low, appropriate heat up).PH=1.6 that coupling starts, coupled processes control PH≤4.2, coupling end pH≤
4.2. after being coupled, the excessive situation of diazo component and coupling component is detected.Then reserved AS-PH solution is added, if
Diazonium does not disappear still within 20 minutes, then continues to add reserved AS-PH, until diazonium disappears.Stirring 15 minutes, then with adjusting hydrochloric acid
PH=3.8 are adjusted, then adjustment motor speed 35HZ is warming up to 97 DEG C of T >, after heat preservation 60 keeps the temperature minute with steam, (period temperature
Greater than 97 degree, open steam and add water 1500L) until annesl is completed.Then 75 DEG C are cooled to, finished product is obtained.
Embodiment 2
Diazo liquid preparation:
It discharges water in diazonium bucket, hydrochloric acid is added, open stirring adjustment motor speed 40HZ, erie Congo base RC42 parts and large red is added
G18 parts of base, 2.5 parts of sodium metnylene bis-naphthalene sulfonate and 3 parts of polysorbas20 stir 15 minutes (inspection is completely dissolved transparent), temperature 27
Degree.Ice adjustment temperature T=1 DEG C is added, sub- 22 parts of sodium is added.It (is detected with KI test paper in the case where keeping the micro- excessive situation of sub- sodium
Micro- aobvious blue) stirring 30 minutes, temperature is controlled at 7 DEG C.Volume 6500L, wait be coupled.
Coupling solution preparation:
Water 5700L is added in dissolving bucket, opens stirring adjustment motor speed 40HZ, is warming up to 47 DEG C with steam, adds azoic coupling component
25 parts of AS-PH, 8 parts of liquid alkaline are added, is dissolved 20-30 minutes, whether detection dissolution is transparent, and dissolution is fully transparent, and diatomite is added
5 parts, 1500 L of water is added to adjust 40 degree of temperature, wait be coupled.
Coupling and heat preservation:
7500 L of water is added in coupling bucket, opens stirring, adjusts motor speed 25HZ, has corrected acidometer, sequentially added liquid alkaline 8
Part and 3 parts of polyoxyethylenealkylphenol ether, pH=4.1, then adjustment temperature on the rocks is extremely, 10 DEG C.Diazo liquid is put into coupling bucket again,
PH=1.6 are adjusted micro- excessive or not excessive to sub- sodium with 3 parts of sulfamic acid.
Coupling is pumped into filter press to be filtered, then it is added to coupling bucket in a manner of being coupled under liquid, adjustment motor turns
Fast 50HZ starts to be coupled.Coupling time requires to be 1.8 hours.It is coupled start temperature and requires 11 DEG C, terminating temperature requirement is about 25
DEG C (if room temperature is too low, appropriate heat up).PH=1.6 that coupling starts, coupled processes control PH≤4.2, coupling end pH≤
4.2. after being coupled, the excessive situation of diazo component and coupling component is detected.Then reserved AS-PH solution is added, if
Diazonium does not disappear still within 20 minutes, then continues to add reserved AS-PH, until diazonium disappears.Stirring 15 minutes, then with adjusting hydrochloric acid
PH=3.9 are adjusted, then adjustment motor speed 35HZ is warming up to 97 DEG C of T >, after heat preservation 60 keeps the temperature minute with steam, (period temperature
Greater than 97 degree, open steam and add water 1500L) until annesl is completed.Then 75 DEG C are cooled to, finished product is obtained.
Embodiment 3
Diazo liquid preparation:
It discharges water in diazonium bucket, hydrochloric acid is added, open stirring adjustment motor speed 40HZ, erie Congo base RC50 parts and large red is added
G25 parts of base, 3 parts of sodium metnylene bis-naphthalene sulfonate and 4 parts of polysorbas20 stir 15 minutes (inspection is completely dissolved transparent), temperature 30
Degree.Ice adjustment temperature T=2 DEG C are added, sub- 30 parts of sodium is added.It (is detected with KI test paper in the case where keeping the micro- excessive situation of sub- sodium
Micro- aobvious blue) stirring 30 minutes, temperature is controlled at 10 DEG C.Volume 6500L, wait be coupled.
Coupling solution preparation:
Water 5700L is added in dissolving bucket, opens stirring adjustment motor speed 40HZ, is warming up to 50 DEG C with steam, adds azoic coupling component
30 parts of AS-PH, 10 parts of liquid alkaline are added, is dissolved 20-30 minutes, whether detection dissolution is transparent, and dissolution is fully transparent, and diatom is added
8 parts of soil adds 1500 L of water to adjust 40 degree of temperature, wait be coupled.
Coupling and heat preservation:
7500 L of water is added in coupling bucket, opens stirring, adjusts motor speed 25HZ, has corrected acidometer, sequentially added liquid alkaline
10 parts and 4 parts of polyoxyethylenealkylphenol ether, pH=4.2. again adjustment temperature on the rocks to 12 DEG C.Diazo liquid is put into coupling bucket again,
PH=1.6 are adjusted micro- excessive or not excessive to sub- sodium with 5 parts of sulfamic acid.
Coupling is pumped into filter press to be filtered, then it is added to coupling bucket in a manner of being coupled under liquid, adjustment motor turns
Fast 50HZ starts to be coupled.Coupling time requires to be 2 hours.It is coupled start temperature and requires 12 DEG C, terminating temperature requirement is about 25 DEG C
(if room temperature is too low, appropriate to heat up).PH=1.6 started are coupled, coupled processes control PH≤4.2, and coupling terminates pH≤4.2.
After coupling, the excessive situation of diazo component and coupling component is detected.Then reserved AS-PH solution is added, if 20 points
Clock diazonium does not disappear still, then continues to add reserved AS-PH, until diazonium disappears.Stirring 15 minutes, then adjusted with hydrochloric acid is adjusted
Then pH=4.0, adjustment motor speed 35HZ are warming up to 97 DEG C of T > with steam, after heat preservation 60 keeps the temperature minute, (period temperature is greater than
97 degree, open steam and add water 1500L) until annesl is completed.Then 75 DEG C are cooled to, finished product is obtained.
Exemplary illustration is carried out to the embodiment of the present invention above, but the content is only preferable implementation of the invention
Example, should not be considered as limiting the scope of the invention.All the changes and improvements etc. of all application ranges according to the present invention,
It should all fall within the scope of the patent of the present invention.
Claims (10)
1. a kind of permanent bordeaux pigment suitable for baking finish, which is characterized in that by weight include following component: 15-25 parts of color base,
20-30 parts of Naphthol AS-PH, sub- 15-30 parts of sodium, 7-10 parts of liquid alkaline, 15-20 parts of hydrochloric acid, 2-4 parts of polyoxyethylenealkylphenol ether,
3-8 parts of diatomite, 2-5 parts of sulfamic acid and 3-7 parts of auxiliary agent.
2. a kind of permanent bordeaux pigment suitable for baking finish as described in claim 1, it is characterised in that: further include 60-80 parts of water
With 45-60 parts of ice.
3. a kind of permanent bordeaux pigment suitable for baking finish as described in claim 1, it is characterised in that: the color base presses mass parts
Including RC35-50 parts and large red-based g 10-25 parts of erie Congo base.
4. a kind of permanent bordeaux pigment suitable for baking finish as described in claim 1, it is characterised in that: the auxiliary agent presses mass parts
Including 2-3 parts and polysorbas20 1-4 parts of sodium metnylene bis-naphthalene sulfonate.
5. a kind of permanent bordeaux pigment suitable for baking finish as claimed in claim 4, it is characterised in that: in the polysorbas20 molecule
Introduce the carboxyl in negative point.
6. a kind of permanent bordeaux pigment suitable for baking finish as described in claim 1, it is characterised in that: the Asia sodium is nitrous acid
One of sodium and sodium sulfite or two kinds.
7. a kind of preparation method of permanent bordeaux pigment suitable for baking finish as claimed in any one of claims 1 to 6, feature
It is: the following steps are included:
(1), the preparation of diazo liquid: it is separately added into color base, auxiliary agent and sub- sodium in acidic environment, diazo reaction occurs, obtain diazonium
Liquid；
(2), the preparation of coupling solution: Naphthol AS-PH, liquid alkaline and diatomite are added into water, obtains coupling solution after to be dissolved；
(3), it is coupled: after coupling solution, polyoxyethylenealkylphenol ether, sulfamic acid is added into diazo liquid, being coupled, obtained
Coupling product；
(4), it keeps the temperature: coupling product being kept the temperature, product is obtained after heat preservation.
8. a kind of preparation method of the permanent bordeaux pigment suitable for baking finish as claimed in claim 7, it is characterised in that: step
(1) whole process needs lasting stirring, stirring rate 40HZ in, and coupling solution temperature is 5-10 DEG C.
9. a kind of preparation method of the permanent bordeaux pigment suitable for baking finish as claimed in claim 7, it is characterised in that: step
(2) solution temperature is 45-50 DEG C in, and the dissolved stand-by temperature of preservation is 38-42 DEG C.
10. a kind of preparation method of the permanent bordeaux pigment suitable for baking finish as claimed in claim 7, it is characterised in that: step
(3) the coupled processes pH in is to add azoic coupling component less than or equal to 4.2, and pH is 3.8-4.0 after diazonium disappears.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811397633.5A CN109439015B (en) | 2018-11-22 | 2018-11-22 | Permanent red pigment suitable for baking paint and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811397633.5A CN109439015B (en) | 2018-11-22 | 2018-11-22 | Permanent red pigment suitable for baking paint and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN109439015A true CN109439015A (en) | 2019-03-08 |
| CN109439015B CN109439015B (en) | 2020-08-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811397633.5A Active CN109439015B (en) | 2018-11-22 | 2018-11-22 | Permanent red pigment suitable for baking paint and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5176750A (en) * | 1991-11-27 | 1993-01-05 | Hoechst Celanese Corporation | Azo pigment compositions and process for their preparation |
| CN1188123A (en) * | 1997-01-13 | 1998-07-22 | 化学工业部沈阳化工研究院 | Red organic pigment and its use |
| CN103468022A (en) * | 2013-08-07 | 2013-12-25 | 中钞油墨有限公司 | Blue azo pigment preparation method |
| CN107163614A (en) * | 2017-06-06 | 2017-09-15 | 宣城英特颜料有限公司 | A kind of permanent bordeaux pigment and preparation method thereof |
-
2018
- 2018-11-22 CN CN201811397633.5A patent/CN109439015B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5176750A (en) * | 1991-11-27 | 1993-01-05 | Hoechst Celanese Corporation | Azo pigment compositions and process for their preparation |
| CN1188123A (en) * | 1997-01-13 | 1998-07-22 | 化学工业部沈阳化工研究院 | Red organic pigment and its use |
| CN103468022A (en) * | 2013-08-07 | 2013-12-25 | 中钞油墨有限公司 | Blue azo pigment preparation method |
| CN107163614A (en) * | 2017-06-06 | 2017-09-15 | 宣城英特颜料有限公司 | A kind of permanent bordeaux pigment and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN109439015B (en) | 2020-08-14 |
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